Apparatus for regenerating a fluidized catalyst



July 22, 1952 L. E` BORDER ET Al.

APPARATUS FOR REGENERATING A FLUIDIZED CATALYST Filed OCL. 5l, 1949 2 SHEETS--SHEE'I' l REGENERATED CATALYST July 22, 1952 l.. E. BORDER ET AL 2,504,384

APPARATUS FOR REGENERATING A FLUIDIZED-CATALYST Filed oct. 51, 1949 2 SHEETS- SHEET 2 STRPPED PRODUCTS REGENERATED CATA LYST Fig. m

nven-lfors: Lawson 55m-der- Their' Hor-neg iatentecl .ul'y 2x2, i952I UNITED STAT-Es Param orricr.

APPARATUSFOR REGENERATING A FLUIDIZED CATALYST Lawson -E.' "BordcnjWestwood, 4'N'. L'J.,' and Richard P l Trainer, Amityville, N. Y., assignorsvto Shell Development Company, San Francisco, Calif., a corporation of Delawa1'ev Application October 31, 1949, Serial No`. 12,4.674

2 Claims.: (Cl. 23,--288) This-invention'relates to an improved methodl and apparatus- `for the continuous regeneration of powdered catalyst and other similar solidcontact material contaminated with -carbonaceous depositsthrough the burning on of theacar bonaceous matter with` an oxygen-containing gas.

An object of` the invention is tovprovdeva. method and apparatus for the regeneration4 of such contact agents in which the oxygen requiredto remove thecarbonaceousdeposits V1s materially decreased. A further object ofthe invention is to provide a method and apparatus which allow valuable products to be recovered from the contaminated solid. Aiurther object ci the invention is `to provide a method and ap.

paratus in which the regeneration may be .car-

ried out in a more convenient andpractical manneron a large scale.

In the treatment of hydrocarbons or othercorbonaceous materials in either the` liquid phase or the vapor phase withnely divided soldcontact materials, the contact material losesits efciency due to contamination with carbonaceous deposits and therefore requires frequent regeneration. In practice the regeneration is .effected by burning the carbonaceous matter under conVv conventional microporous catalysts such as used in the catalytic cracking, catalytic reforming, hydroforming, polymerization, and refining of hydrocarbon oils. The process `and apparatus are applicable, however, for the regeneration of other micrcporous (adsorptive) solid Contact agents whether acting in the true catalytic sense.

or not, and regardless ci the process in which they became contaminated with carbonaceous deposits. Thus, they are quite suitable for the regeneration of decolorizing clays and similar contact agents used in the treatment of vege' table oils, animal oils, chemical intermediates and the like. The contact agent should, however, be in a sufficiently nely divided state to be handled by the known luidized solid technique. It is preferred that the majority of the particles of the solid pass through -a Astandard -(U.A Si.) 40-` mesh sieve.

2 The contact agent at use contains appreciable amounts of the material treated, either in the liquid phase, the vapor l This material is to a phase, or both phases.y large extent occluded, i. e., it is present-in the voids betweenthe particles and in the pores of the particles. Prior to burning the carbonaceous material from the particles, it is the practice to Y replace such occluded material with a relatively inert "material, and :this step is commonly known as stripping gas such as steam, ilue gas. nitrogen-or the like is passed through a bed of the contact material to displace and remove most of the occluded car- The resulting stripped mate bonaceous matter. rial is then subjected to the burning treatment.

In the burning treatn'ientY it is the practice to pass the oxygen-containing gas-(commonly Are ferred to as the regeneration gas)` up througha bed of the contact material at a rate adj-usted to maintain the iinely vdivided solid'in the "so`Y called uidized or pseudo liquid state. The maximum gas velocity which can be Aappliedwhile still maintaining the pseudo liquid condition depends, as known; uponvthe density, shape, and v neness of the particles, but the velocity applied is usually in 'the order of one-to--two--feet per second (calculated on the basis ofthe vessel without the fiuidized solid present; i. e. super flcial gas velocity). The operation caribe-carried out in either of two ways which may be designated upflow and downlow, depending upon the type of regenerator used. In the upow sys-` tem the regenerated material is withdrawny from the regenerator overhead as a dilute suspension- (dust cloud) in the spent regeneration gas and f' is subsequently recovered. In lthe downlow system the regenerated material is withdrawn as a dense, pseudo liquid, directly from the iiuidized bed. The down now type system is superior.A

The present invention relates type of system.

In the process of this invention the operation iscarried out in two separate zonesv which are particularly to this Vin direct communication near their lower extremities in such a manner as to resemble a U.

The finely divided solid is maintained in a pseudo liquid condition in both zones. The contaminated material from which the occluded car- 2bonaceous material has preferably been previously removed, is introduced near the top of one zone and the regenerated material is withdrawn from near the top of the other zone. Gas is in'- trodu'ced into eachzone near the Ibottom and 55;V @the-gases leaving Athe 4top ofthe uidized bed in the end of -a period oi` In stripping, a relatively inert each zone are separately withdrawn. Aside from the flow of solid material from the bottom of the rst zone to the bottom of the second zone there is maintained a circulation of solid material from the second zone to a higher point in the first zone. This circulation is effected by injection through inclined, restricted passages using a portion of the required gas for the purpose.

Having set forth the operation in general terms, the method and apparatus will be more particularly described in connection with the accompanying drawings wherein Figure I shows an elevation in cross section of an apparatus designed for operation according to the method of the invention.

Figure II shows an elevation in cross section of a modified apparatus also designed to operate according to the method of the invention.

Figure III shows a sectional plan of the apparatus illustrated in Figure II, the section being taken through IIL-III.

Figure IV shows the details of one -modiiication of injector such as may be applied in the apparatus of Figures I, II and VI.

Figure V shows in cross section the details of a second modification of a gas injection tube such as may be substituted for that illustrated in Fig. IV.

Figure VI shows in cross section the pertinent part of an elevational View in cross section of an apparatus such as illustrated in Figure II modified through the use of extended injection tubes.

Referring to Figure I of the drawing, the apparatus comprises two cylindrical vessels, I and 2, swaged near their upper ends to a larger diameter and communicating near their bottom ends. The two vessels are of different horizontal cross section but substantially coextensive in elevation. Each vessel is provided with a separator 3, 4 for separating dust from the eiuent gases. Each separator is provided with a dip leg 5, 6 which extends downwardly to a point below the normal level of the pseudo liquid bed, indicated by lines 1 and 8. Each vessel is also provided with means for injecting gas near the bottom. In vessel I this is a grid of perforated pipe 9 communicating with the gas inlet line ID. In vessel 2 a horizontal grid I I is provided to distribute the gas introduced at the bottom of the vessel via line I2. Vessel I is provided with an inlet line I3 for the introduction o f the contaminated contact material. This line is arranged to discharge the contaminated material at a point near the upper level of the pseudo liquid bed. Vessel 2 is provided with a line I4 for the withdrawal of the regenerated solid. This line is arranged to withdraw the solid as a pseudo liquid from a point near the upper level of the pseudo liquid bed. Vessels I and 2 are also interconnected by a series of inclined pipes I5 having their lower ends in vessel 2 at points below the level of the pseudo liquid bed and having their upper ends at higher points in vessel I, also below the level of the pseudo liquid bed. A series of nozzles I6 are arranged to cooperate with the inclined tubes as will be explained. These nozzles are fed with gas from a manifold line II which enters through the bottom of the larger vessel.

In operation, the powdered contact material contaminated with carbonaceous deposits, but preferably stripped of most of the occluded carbonaceous material, enters the apparatus via line I3 in a substantially continuous stream. The nely divided solid ows downwardly and then laterally to a point near the bottom of Vessel 2;' it then flows upwardly through vessel 2 and is finally withdrawn through the discharge line I4.

An important feature of the method of the in-4 vention is that, aside from the desired flow in the roughly U shaped path, a substantial, although minor, portion of the finely divided solid is continuously injected from the second zone up through the inclined passages to the first zone. This flow is caused to take place and is regulated by the gas introduced via line I1 and nozzles I6. In order to obtain this flow it is essential that the passages be inclined, and in order that the full benet of this invention may be realized it is necessary that a plurality of such pipes be provided.

In the described method as carried out in the apparatus illustrated in this figure, the contact f material ows downwardly in the rst cell in admixture with partially regenerated contact material injected through the inclined passages and countercurrent to the gas introduced via line I0 and that introduced via the inclined passages. The gas introduced va line IIJ may be a relatively inert gas such as steam, flue gas, nitrogen, carbon dioxide or the like, or it may contain a small amount of oxygen insucient to burn the carbonaceous deposits. The gas introduced via the inclined tubes may be the same or different than that introduced via line I0. Thus, for example, steam or carbon dioxide may be introduced via line IU and air or oxygen may be introduced via lines I5. In the first zone, due to the countercurrent contact, the injection of the partially regenerated catalyst from the second zone,

and the relatively inert nature of the gas used, the carbonaceous deposits in the solid are largely removed with little actual combustion. The temperature in this first zone is preferably maintained between 750 F. and 1000 F. This temperature may be maintained by heating means (not shown), or by preheating the incoming contact material, or by preheating the gas, or by regulating the oxygen content of the gas to aiord a desired minor amount of combustion, or by any combination of these means, but part of the heat is supplied by the partially regenerated material injected as described. In the usual practice, the heat is supplied by a combination of these means, namely, by supplying the solid in a heated condition, using hot gases, applying a very limited combustion, and by the heat supplied by the injected solid. Even though the residence time of the solid in the first zone is short compared to that in the second zone, a substantial part of the carbonaceous deposits may be removed with little or no combustion. The gas leaving the iirst zone via line I8 is suitable as a fuel gas and in many cases it is also possible to recover product values from it by cooling and/or scrubbing with a suitable solvent. It is also possible, although wasteful, to combine the gases from this zone with the flue gas from the second zone.

In the second zone the partially regenerated solid passes upwardly concurrent with the gas introduced Via line I2. This gas is usually air, but may be industrial oxygen or any other gas containing suiiicient oxygen to burn the carbonaceous deposits to the desired extent. The temperature in the second zone is maintained higher than that in the rst zone and is preferably in the rangeof 1.000u F. to 1200o F. In some cases a small amount (e. g. 0.02 to 1%) of a volatile halogen compound, such as carbontetrachloride, phosgene, sulfur pentachloride, dichloropropane, hydrogen chloride, or the like, may be advantageously introduced with the gases via line |2. In some cases the presence of these or similar halogen compounds changes the combustion characteristics so that the production f carbon monoxide rather than carbon dioxide is favored. This results in a decreased liberation of heat and, therefore, allows a greater gas velocity and/or a higher concentration of oxygen to be used without exceeding the desired temperatures.

The apparatus illustrated in Figure II employs the same flow system and the same system of catalyst injection as that illustrated in Figure I described above. The main difference is in the construction of the apparatus. Whereas the apparatus of Figure I comprises two cylindrical vessels at approximately the same elevation spaced a small distance apart, that illustrated in Figure II contains both zones in a single cylindrical housing, the separate zones being formed by a vertical partition 2| which extends from-the top of the vessel to a point near, but short of, the bottom. This construction has the further advantage that a larger number of inclined tubes 22 may be conveniently spaced in the partition to obtain a more uniform distribution of the injected solid in the first zone. Thus, in a typical case, from 6 to 30 or more such inclined tubes may be placed in the partition without difficulty due to crowding or expansion problems. While the apparatus illustrated in Figure II is no more efficient (considering an equal number of inclined tubes properly spaced) it is considerably simpler and less costly to build.

In the apparatus illustrated in Figure II a perforated coil 23 is provided to distribute the gases introduced into the second zone via line 24, rather than a grid such as illustrated in Figure I. It will be noted that in this structure the gas distributing devices are located near the bottom of the separate zones but at such a distance from the bottom that the gases remain separated by the depending partition.

As stated above, part of the required gas is utilized in the present process to inject solid from the second zone to the rst zone through inclined passages. When both ends of the inclined passages (tubes) terminate below the levels of the nuidized beds as illustratedv in Figures I and II, it is essential that the passages be inclined at an appreciable angle, e. g. about 45, in order to obtain the desired flow. The gas may be directed up through the tubes by means of nozzles placed at their lower openends. preierably inserted a few niches. Some diiilculty may be incurred in starting the ow with suon nozzles without using a very high gas velocity (pressure). In order to overcome this dlculty, centered, perforated pipe extending over a considerable part of the length of the tubes may be used instead of nozzles. Such an arrangement is illustrated in Figure V. The minor amount of gas inJected by the few upper periorations aids considerably in starting the oW. A preferred modification, however, uses a combination of the nozzle and the centered perforated pipe. Such a modifi-cation is illustrated in Figure IV. In this arrangement the main quantity of the gas introduced via line 4| passes into the tube 42 at the mouth via the nozzle 43. A minor portion of the gas passes up through the centered tube and is discharged via outlets 44 at higher points in the tube 42.

In the apparatus illustrated in Figures I and II, the upper ends of the inclined tubes discharge below the level of the fluidized bed in the first zone. The injection of powdered solid through a plurality of inclined tubes in this manner produces a quite uniform distribution of the injected solid in the contaminated solid passing down through the rst zone. This is desirable. On the other hand, the control of the flow in this system is rather Isensitive to fluctuations in the system and is somewhat difficult.

A system which is more easily controlled is illustrated in Figure VI. The apparatus in this case is the same as that illustrated in Figure II, except for the differences noted in the section shown. In this system the inclined tubes are extended in a Vertical direction to discharge into the upper so-called disengaging space above the level of the liuidized bed. A baille 6| is preferably provided to deflect the discharged solid in a downward direction. If such a baille is not provided a considerable amount of the solid may escape from the apparatus with the gases withdrawn via line 62.

The claimed invention is:

1. An apparatus for the regeneration of contaminated powdered contact agents which comprises a vertical regenerator shell closed at the top and bottom, a depending partition member extending from the top to a point short of the bottom. outlets for gaseous iiuid on each side of said partition member at the top, inlet for contaminated powder near the top on one side of said partition member, an outlet for regenerated powder near the top on the other side of said partition member, a plurality of inclined conduits extending through said partition member, a pluralitylof gas jets in cooperative relationship to the lower ends of said inclined conduits, and gas distributing means near the bottom on either side of said partition member.

2. Apparatus according to claim 1 further characterized in that said inclined conduits are extended at their upper ends in an upward direction with their discharge ends below a deecting plate near the top on the intake side of said partition.

LAWSON E. BORDER. RICHARD P. TRAINER.

REFERENCES CITED The following references are of record in the le of this patent:

UNITED STATES PATENTS Number Name Date 2,429,721 Jahnig Oct. 28, 1947 2,457,232 Hengstebeck Dec. 28, 1948 2,477,751 Johnson Aug. 2, 1949 2,526,881 Kunreuther et al. Oct. 24, 1950 2,571,380 Penick Oct. 16, 1951 

1. AN APPARATUS FOR THE REGENERATION OF CONTAMINTED POWDERED CONTACT AGENTS WHICH COMPRISES A VERTICAL REGENERATOR SHELL CLOSED AT THE TOP AND BOTTOM, A DEPENDING PARTITION MEMBER EXTENDING FROM THE TOP TO A POINT SHORT OF THE BOTTOM, OUTLETS FOR GASEOUS FLUID ON EACH SIDE OF SAID PARTITION MEMBER AT THE TOP, INLET FOR CONTAMINATED POWDER NEAR THE TOP ON ONE SIDE OF SAID PARTITION MEMEBER, AN OUTLET FOR REGENERATED POWDER NEAR THE TOP ON THE OTHER SIDE OF SAID PARTITION MEMBER, A PLURALITY OF INCLINED CONDUITS EXTENDING THROUGH SAID PARTITION MEMBER, A PLURALITY OF GAS JETS IN COOPERATIVE RELATIONSHIP TO THE LOWER ENDS OF SAID INCLINED CONDUITS, AND GAS DISTRIBUTING MEANS NEAR THE BOTTOM ON EITHER SIDE OF SAID PARTITION MEMBER. 